主题：【分享】50.10液相色谱测定三乙醇胺酯及酯季铵盐的组成分布

[作者]宫志鹏
[摘要]:建立了反相高效液相色谱法测定三乙醇胺酯中单、双、三酯含量的方法。采用Diamonsil C18色谱柱(250X4．6mm，5I，tm)，柱温30。C，溶剂为氯仿，流动相为甲醇和氯仿，检测器为电雾式检测器。通过讨论k’值和兄与流动相极性、流速和柱温的关系，确定了梯度洗脱程序，30rain内三乙醇胺单、双、三酯得到了较好的分离。三乙醇胺单、双、三酯在20．500mg·L．1范围内线性关系良好，线性相关系数分别是0．9980、o．9991和0．9913，最低检出质量浓度分别(3s／N)是1．0mg·L～、1．5mg·L-1和1．5mg·L-1，相对标准偏差(n=6)分别是2．45％、1．81％ 和1．98％。优化了反相高效液相色谱测定三乙醇胺酯季铵盐中单、双酯混合季铵盐与三酯季铵盐含量的方法。样品经过乙醚萃取处理，采用Inertsil CN．3色谱柱(250× 4．6ram，5Irtm)，柱温50。C，溶剂为正丙醇，流动相为正丙醇和水，梯度洗脱， 检测器为电雾式检测器，并采用液相色谱．质谱法确证，15min内三乙醇胺单、双酯混合季铵盐与三酯季铵盐得到了较好的分离。单、双酯混合季铵盐与三酯季铵盐在25．750mg·L。1范围内线性关系良好，线性相关系数分别是O．9966和O．9913，检出F艮(3s／y)是0．8mg·LJ和10．0mg·L一，相对标准偏差(n=6)分别是0．5 l％和12．38％。
[关键词]：三乙醇胺酯，三乙醇胺酯季铵盐，梯度洗脱，高效液相色谱，电雾式检测器

Abstract :An analytical method of reversed phase hi曲performance liquid chromatography(RP-HPLC)was developed for determination of triethanolamine mono-，di—and triesters．Established a gradient elution programme by analyzing the relationship of k’，R and elution rate，elution polarity,temperature． Triethanolamine mono-，di-and triesters were detected and separated successfully by Diamonsil Cls column(250x4．6mm，59m)and column temperature of 30"C，with chloroform as solvent and methanol-chloroform as the mobile phase in gradient elution and with a Charged aerosol deteror．The linear ranges of triethanolamine mono一，di-and triesters were 20-500 mg‘L。(r=O．9980)，20-500 mg·L。1(r=0．9991)and 20—500mg‘L_(r=0．9913)respectively．The measurable lowest limits were 1．0rag‘L一， 1．5mg’L—and 1．5mg‘L—and the RSDs were 2．45％．1．8 1％and 1．98％respectively． An analytical method of reversed phase hi曲performance liquid chromatography(RP—HPLC)was optimized for determination of triesterquats in 1 5min．Mono-，diesterquats mixture and triesterquats were detected and separated ccessfully by Inertsil CN一3 column(250x4．6mm，5pm)and column temperature of 30。C．with n—propanol as solvent and n—propanol—water as the mobile phase in gradient elution and with a charged aerosol deteror．The linear ranges of mono一， diesterquats mixture and triesterquats were 25-750mg·L-1(FO．9966) and 25-750mg’L叫(r=0．9913)respectively．The measurable lowest limits were 0．8mg‘L。1 and 10．0mg。L-1 and theRSDs were 0．51％and 12．38％respectively． Key words：triethanolamine esters，esterquats，gradient elution，high performance liquid chromatograph，charged alesol detection